The invention discloses a treatment method of complexing nickel wastewater. Compared with the prior art, Fe is loaded on granular active carbon, and a supported Fe2O3.FeO / GAC catalyst is prepared, a heterogeneously activated persulfate system generates sulfate radical free radicals with the strong oxidizing property to oxidize complex form heavy metals in the wastewater, by damaging the stable structure of complexing ions, the heavy metals are freed from complex, and the heavy metals are removed through a simple alkaline chemical precipitation method. The Fe2O3.FeO / GAC activated persulfate coupling system is established, the pH value of the wastewater is adjusted through the actual condition of the wastewater during wastewater treatment, a good treatment effect can be achieved, the catalyst still has good catalytic activity after being reused, and the wastewater treatment cost can be greatly reduced. A large amount of equipment investment and operating cost is not needed, materials are easy to take, and operation is simple. The active carbon carrier can be reused, resource reuse is achieved, and cost is reduced.